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Development of a Microelectrode Array Sensing System for Water Quality Monitoring Utah State University DigitalCommons@USU All Graduate Theses and Dissertations Graduate Studies 5-2008 Development of a Microelectrode Array Sensing System for Water Quality Monitoring Robert D. Gardner Utah State University Follow this and additional works at: https://digitalcommons.usu.edu/etd Part of the Chemical Engineering Commons Recommended Citation Gardner, Robert D., "Development of a Microelectrode Array Sensing System for Water Quality Monitoring" (2008). All Graduate Theses and Dissertations. 648. https://digitalcommons.usu.edu/etd/648 This Thesis is brought to you for free and open access by the Graduate Studies at DigitalCommons@USU. It has been accepted for inclusion in All Graduate Theses and Dissertations by an authorized administrator of DigitalCommons@USU. For more information, please contact [email protected]. DEVELOPMENT OF A MICROELECTRODE ARRAY SENSING SYSTEM FOR WATER QUALITY MONITORING by Robert D. Gardner A thesis submitted in partial fulfillment Of the requirements for the degree of MASTER OF SCIENCE in Biological Engineering Approved: ________________________________________ ________________________________________ Dr Anhong Zhou Dr James W. Burns Major Professor Committee Member ________________________________________ ________________________________________ Dr Ronald Sims Dr Byron R. Burnham Committee Member Dean of Graduate Studies UTAH STATE UNIVERSITY Logan, Utah 2008 ii Copyright © Robert Gardner 2008 All Rights Reserved iii ABSTRACT Development of a Microelectrode Array Sensing System for Water Quality Monitoring by Robert D. Gardner, Master of Science Utah State University, 2008 Major Professor: Dr. Anhong Zhou Department: Biological and Irrigational Engineering This thesis reports the design and fabrication of a low‐cost reliable microelectrode array sensing platform and its application toward water quality monitoring, including heavy metal ion detection. Individually addressable microelectrodes were designed in a planar array on a nonconductive glass substrate by a photolithography method. The size, shape, composition, and functionality of the microelectrodes were theoretically explored in order to maximize performance. The microelectrode array sensing platform was proven and characterized in the K3Fe(CN)6 electrochemical standard using cyclic voltammetry. The sensor platform exhibited well defined voltammograms and had increased sensitivity relative to a commercially available microelectrode of similar size. Feasibility for application to heavy metal ions, copper and lead, detection in aqueous solutions was demonstrated utilizing the electrochemical method of anodic stripping voltammetry. Well defined voltammograms for the copper and lead ions were obtained with individual microelectrodes of the sensor platform, and compared against the similar sized commercially available microelectrode; increased sensitivity was observed. iv Finally, a piecewise proving technique was done to prove the feasibility for future coupling of the microelectrode array sensor platform with a previously developed homemade electrochemical device. By analyzing the response of the homemade electrochemical device compared to that of a commercially available electrochemical analyzer, feasibility was demonstrated. (153 pages) v ACKNOWLEDGMENTS I would like to especially thank Dr. Anhong Zhou for being my advisor, mentor, and friend throughout my time working in his lab and on this thesis. I would like to thank my committee members, Dr. Ronald Sims and Dr. Jim Burns, for their valuable assistance, thoughts, and inspiration for completion of this project. I am also grateful the financial supports from Utah Water Research Laboratory (UWRL), National Institute of Health, USU College of Engineering, and the Dean’s Office Teaching Funds. I also thank the lab colleagues from Dr. Zhou’s lab for their help during my studies. I would like to express my gratitude to Brian Baker from the MicroFab Lab at University of Utah to provide me with great help with the training and use of their microfabrication facilities there. I am thankful to Dr. Yangquan Chen and his lab, especially Mr. Austin Jenson, who helped a lot with the setup of homemade SWV box. I would like to especially thank my wonderful family, friends, and colleagues who have supported me throughout the duration of this project; they never tired of helping me. My strongest gratitude is reserved for Patricia Korey; thank you for being so patient with me. Robert Gardner vi CONTENTS Page ABSTRACT ........................................................................................................................................................ iii ACKNOWLEDGMENTS .................................................................................................................................. v CONTENTS ....................................................................................................................................................... vi LIST OF TABLES ............................................................................................................................................. ix LIST OF FIGURES ............................................................................................................................................. x CHAPTER 1 PROJECT INTRODUCTION .................................................................................................................. 1 1.1 Problem Description ....................................................................................................... 1 1.2 Overview of the Solution ............................................................................................... 2 1.2.1 Stripping Voltammetry Analysis ............................................................. 3 1.2.2 Square Wave Anodic Stripping Voltammetry (SWASV) and Differential Pulse Anodic Stripping Voltammetry (DPASV) .............. 4 1.2.3 Microelectrode and Nonlinear Diffusion ............................................. 5 1.2.4 Combination of Voltammetry and Microelectrode .......................... 7 1.3 Aims ........................................................................................................................................ 7 1.4 Outline of Technical Contents ...................................................................................... 8 2 DESIGN AND CHARACTERIZATION ............................................................................................... 9 2.1 Voltammetric Criteria for Testing Utilizing Microelectrodes ......................... 9 2.2 Experimental .................................................................................................................... 14 2.2.1 Photolithography Fabrication of MEA ................................................ 14 2.2.2 MEA Sensor Fabrication and Construction ....................................... 16 2.2.3 Electrochemical Measurements and Reagents ............................... 18 2.3 Results and Discussion ................................................................................................. 20 2.3.1 Comparison of CV Results of MEA Microelectrode and 2 mm Au Electrode ............................................................................................................... 20 2.3.2 Repeatability of CV Results for Single MEA Electrode ................. 22 2.3.3 Repeatability of 18 MEA Electrodes in 0.3 mM and 0.5 mM K3Fe(CN)6 Solutions ......................................................................................... 23 2.3.4 Comparison of CV Results for MEA Electrode and 10 μm CH Electrode in Different K3Fe(CN)6 Solutions ............................................ 29 vii 2.3.5 Comparisons of SWV Results for MEA Electrode and 10 μm CH Electrode ............................................................................................................... 35 2.4 Conclusions ....................................................................................................................... 38 3 STRIPPING ANALYSIS FOR COPPER AND LEAD IONS .......................................................... 39 3.1 Stripping Analysis and Testing Criteria ................................................................. 39 3.2 Experimental .................................................................................................................... 42 3.3 Results and Discussion ................................................................................................. 44 3.3.1 DPASV Detection of Cu Ion Solutions by MEA Electrode ............ 44 3.3.2 SWASV Detection of Cu Ion Solutions by MEA Electrode ........... 51 3.3.3 DPASV Detection of Pb Ion Solutions by MEA Electrode and 10 µm CH Electrode ................................................................................................ 53 3.3.4 SWASV Detection of Pb Ion Solution by MEA Electrode and 10 µm CH Electrode ................................................................................................ 56 3.3.5 Effect of Reversing Potential Direction on Cu and Pb Stripping Analysis ................................................................................................................. 59 3.4 Conclusions ....................................................................................................................... 67 4 COUPLING WITH ELECTROCHEMICAL CHIP ANALYZER ................................................... 69 4.1 Feasibility in Coupling EC‐Chip Analyzer with the MEA Platform ............
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